Apparatus for determining fluid contents of solids



y 1942- w. L. HORNER 2,282,654

APPARATUS FOR DETERMINING FLUID CQNTENTS 0F SOLIDS Original Filed Jan.'3, 1938 'INVENTOR Walliam L. Home! BY Q r/Q .7 ATTORNE Patented May 12, 1942 APPARATUS FOR DETERMINING FLUID CONTENTS OF SOLIDS William L. Homer, Dallas, Ten, assignor to Core Laboratories, Inc., Dallas, Tex., a corporation of Delaware Original application January 3, 1938, Serial No.

Divided and this application August 8, 1940, Serial No. 351,892

Claims.

The present invention relates to a method and apparatus for distilling liquids from the pores of porous rock or sand, such as comprise core samples taken during the drilling of an oil or gas well, for the purpose of making quantitative determination of the liquids present.

The present application is a division of my copending application Serial No. 183,018, filed January 3, 1938.

One of the objects of the invention is to provide an improved method for making such quantitative determinations and to provide improved apparatus for making such determinations and for carrying out the novel method.

The drawing shows in axial vertical section apparatus embodying the invention.

The still shown in the drawing is adapted to distill oil and water from core samples S and to collect the products of distillation in a graduated tube generally indicated at 2 supported below the still by a connecting tube generally indicated at 4.

The still comprises an insulated heater having an inner chamber 6 adapted to receive a sample container 8. Around chamber 6 is a ceramic shell, such as porcelain and indicated at Ill. The shell is spirally grooved on its outside as shown and is open at its bottom and is closed at its top with a porcelain top [2. Closely fitted inside the porcelain shell is located a polished steel shell l4 having sides and a top and supported at its open bottom by a flange ring I6. Wound around the outside of the grooved porcelain shell is a resistance heating wire l8, and packed around this wire and held in by a suitable metal cover is suitable packing 22, such as magnesium silicate. The top and bottom walls holding the magnesium silicate packing are respectively an asbestos disc 24 and an annular ring 26, respectively, held together by three tie rods 28. The ends of the resistance wire come out through the top 24 and are secured to suitable insulated terminals from which extends a cord adapted to connect the resistance wire with a supply of electricity. As shown in the drawing, the heating mechanism does not extend to the lower part of the steel shell l4 and consequently the lower portion of the shell and the bottom 34 are not heated to the temperatures to which the upper parts of the apparatus are heated.

The annular supporting flange I6 is provided with downwardly-extending bolts 32 for clamping a base plate 34 to the supporting flange. The

' inside of the base plate is conically dished at its center, as shown, and at the apex of the conical iormationis provided an outlet 36 into which i brazed a short bronze tube 38. The outlet tube is connected by suitable rubber connections to a relatively long copper tube 40 serving as a condenser and terminating in a rubber stopper 42 in the top of the graduated glass tube 2. A suitable vent 44 also extends upwardly from the stopper.

The sample container 8 is preferably made of some corrosion resisting material, such as monel metal, or is plated with some-corrosion resisting plating. It is open at its top and has a perforatedbottom. A spacing rod 46 extends downwardly from the container.

In operation the sample container is filled with pieces of core samples that have previously been weighed. While the base cover 34 is removed the container is inserted in the heating chamber 6 and is pushed to the top of the chamber by the spacing rod 46 as the base 34 is moved into its closing position. After the container and sample have been placed in the heating chamber 6 and the base plate 34 bolted in place, the heat is turned on and the sample is eventually heated to a dull red temperature which insures all oil, gas and water being driven off. The oil, which is driven oil in the form of vapors, is always caused to move to cooler regions, and as it passes down through the tube 40 is sufliciently cooled so that it condenses and drips into the graduated tube 2.

During the heating the amount of oil and water collecting in the tube is plotted against time, because the first water that comes oii is the free" water, i. e. the connate water and drillmud water which may be present in the sample. As the heating continues, the water stops coming over for a short time and then commences to come over again. This last water to come over is probably water of crystallization and does not enter into the problem of oil production.

The purpose of plotting the water distilled against time isto be able to read the amount of v total free water distilled from the sample. From the graduations on the tube 2 is obtained the amount of oil that came over and the amount of total water. The weight measurement of the sample put into the chamber 8 may be converted to volume by means of a density measurement made by weighing a corresponding sample and obtaining the volume of the sample by a liquid displacement measurement. Thus from the foregoing readings it is possible to obtain the percentage of oil saturation and the percentage of total water saturation per unit volume of core sample.

The above method of distilling the water and oil from the sample has the advantage of being rapid and accurate. The heavy vapors of the distillate ilow by gravity to the colder regions and the condensing tube. A further advantage of the present method and the apparatus for interpreted as illustrative and not in a limiting sense.

I claim:

1. In apparatus for determining the oil and free water content of core samples, in combination, a distilling chamber defined by top and side sealed metal walls, an outer ceramic shell closely fitting over said metal wall, resistance wire associated with said ceramic shell and adapted to heatmthe same and said metal walls to heat the chamber, a sample container shorter than said distilling chamber open at its top and perforated at'its bottom and adapted to be inserted into said chamber, a bottom cover for closing said distilling chamber, a spacing rod extending between said sample container and said bottom cover and for supporting said sample container from said bottom cover to maintain said sample container in the upper portion of said distilling chamber, the inside surface of said base cover being conically-concavely shaped, an outlet opening downwardly from the apex of said conical surface, a condensing tube extending downwardly from said opening and a container below said tube for collecting the condensate.

2. In apparatus for determining the oil and free water content of core samples through the collection of oil and water distilled therefrom, in combination, a distilling chamber so limited in size as substantially to discharge completely the vapors distilled from small core samples placed therein, said chamber being closed except for a discharge opening in the bottom thereof, means for opening said distilling chamber for aaaaesa walls of said distilling chamber, a condensing tube extending downwardly from but not above said discharge opening, and means for receiving the condensate from said tube.

4. In apparatus for determining the oil and iree water content of core samples by distilling the oil and water therefrom, in combination, a distilling chamber having top, side and bottom walls so limited in size as substantially to discharge completely the vapors distilled from small core samples placed therein, said chamber being closed except for a discharge opening in the bottom wall, means for supplying heat energy at a controlled rate to said side walls, means for opening said distilling chamber to insert core samples therein and for reclosing and sealing said chamber, a condensing tube extending downwardly from but not above said discharge opening, whereby vapors from said sample may move always downwardly to said discharge opening, ant?e means for receiving condensate from said tu 5. In apparatus for determining the oil and free water content of core samples by distilling the oil and water therefrom, in combination, a distilling chamber having top, side and bottom walls so limited in size as substantially to discharge completely the vapors distilled from small core samples placed therein, said chamber being closed except for a discharge opening in the bottom wall, means for supplying heat energy at a controlled rate to said side walls, means for opening said distilling chamber to insert core samples therein and for reclosing and sealing said chamber, a condensing tube extending downwardly from but not above said discharge opening, whereby vapors from said sample may move always downwardly to said discharge opening, and

I means for receiving condensate from said tube,

the insertion of core samplesand for reclosing and sealing said chamber, means for heating the contents of said chamber, a condensing tube extending downwardly from but not above said discharge opening, whereby substantially all vapors moving downwardly from said sample may enter said discharge opening, and means for receiving the condensate from said tube.

3. In apparatus for determining the oil and free water content of core samples by distilling the oil and water therefrom, in combination, a distilling chamber so limited in size as substantially to discharge completely the vapors distilled from small core samples placed therein, said chamber being closed except for a discharge opening in the bottom thereof, the inside bottom surface of said distilling chamber having a concave conical shape and said discharge opening being located at the apex of said conical surface, means for opening said distilling chamber to insert core samples therein and for reclosing and sealing said chamber, means for heating the side and said bottom wall and discharge opening being below the heating means so that the temperature of said bottom wall is maintained below that of the side walls.

6. In apparatus for determining accurately the fluid content of a core sample through the collection of fluid distilled therefrom, in combination, a distilling chamber having top, bottom and side walls, said distilling chamber being so limited in size as substantially to discharge completely the vapors distilled from small core samples placed therein and being closed except for a discharge opening in the bottom wall thereof, the bottom wall of said distilling chamber being removable to insert core samples in said distilling chamber and being replaceable to seal said chamber, a condensing and measuring tube extending downwardly from but not above said discharge opening, and means for supplying heat directly to the side walls of said distilling chamber without applying heat directly to the bottom wall to vaporize the vaporizable material in said core sample which moves downwardly through said discharge opening to said condenser where it is condensed and retained in said measuring tube.

7. In apparatus for determining accurately the fluid content of core samples through the collection of fluid distilled therefrom, in combination, a distilling chamber having top, bottom and side walls and being so limited in size as substantially to discharge completely the vapors distilled from small core samples placed therein, said distilling chamber being closed except for a discharge opening in the bottom wall thereof, a sample container shorter than said distilling chamber, said bottom wall being removable to permit placing said sample container in said distilling chamber, means for holding said sample container in'the upper portion of said distilling chamber spaced from said bottom wall, a condensing tube extending downwardly from but not above said discharge opening, and means for supplying heat to said distilling chamber.

8. In apparatus for determining accurately the fluid content of a core sample through the collection of fluid distilled therefrom, in combinamit placing of said core samples in said distilling chamber, means for holding said sample in the upper portion of said distilling chamber and 10 tion, a distilling chamber having top, bottom and spaced from said bottom wall. and means for heating the upper portion of said distilling chamber to a temperature appreciably higher than that of the bottom wall whereby vapors distilled from said core sample flow downwardly and leave the distilling chamber through a cooler region.

9. In apparatus for determining accurately the fluid content of a core sample through the collection of fluid distilled therefrom, in combination, a

distilling chamber having top, bottom and side walls and being of such size as substantially completely to discharge vapors distilled from the sample placed therein, said distilling chamber being closed except for a discharge opening in the able to permit placing of said sample in said dis-v tilling chamber, and means for supporting the sample in the upper portion of said distilling chamber appreciably spaced from said bottom wall whereby the sample is held in theheated part of said distilling chamber and the vapors from the sample pass downwardly to leave the distilling chamber through a cooler region.

10. In apparatus for determining accurately the fluid content of a core sample through the collection of fluid distilled therefrom, in combination, a distilling chamber having top, bottom and side walls and being of such size as substantially completely to discharge vapors distilled from small core samples placed therein, said distilling chamber being closed except for a discharge opening in the bottom wall thereof, means for opening said distilling chamber to insert core samples therein and for reclosing and sealing said chamber, resistance wire for heating the side walls of said distilling chamber, a condensing tube extending downwardly from but not above said discharge opening, and means below said condensing tube for collecting the condensate therefrom whereby fluid distilled from said core sample may always move downwardly to said collecting means.

WILLIAM L. HORNER. 

